Apparatus for hydrogenating carbonaceous material



Mar. 27, 1923.

T. ULKE.

APPARATUS FOR HYDHOGENATING CARBONACEOUS MATERIAL.

2 SHEETS SHEET 1.

FILED APR; 14. 1922.

anoeul'oz Patented Man. 27,

UNITED STA 'TITUS ULKE, OF WASHINGTON, DISTRICT OE COLUMBIA.

APPARATUS FOR HYDROGENATING CABBONACEOUS MATERIAL.

Application filed April 14, 1922. Serial no, 552,735.

To all whom it may concern: Be it known that I, TI'r s ULKE, a citizen of the United States, residing in the city of Washington, District of Columbia, have invented certain new and useful Improvements in Apparatus for Hydrogenating Carbonaceous Material, of which the following is a specification.

This invention relates to high pressure retorts and has reference particularly to the class of such apparatus employed in treating carbonaceous material, such as peat, lignite,

saw-dust and bituminous coal for the purpose of recovering higher percentages of marketable fluid hydrocarbons therefrom than .are usually obtained, and also to produce other valuable organic compounds.

According to my invention I employ a gas-tight, metal-jacketed cylindrical vessel 2 or retort, of high-pressure-resisting material, mounted on bearings so as to be readily rotatable and provided with an easily manipulable but gas-tight closure, fermeture,

door or plug for a charging and discharg- 5 ing opening and carrying a valve-controlled passage way for fluids; and my chief objects are to effect a rapid and convenient opening I andclosing of the vessel in loading or discharging it, instead of the inconvenient manhole manipulation, as in highpressure re- /tortsnow in use, a convenient mixing of the contents of the vessel wlthout requiringany mechanism within the vessel itself, as in other high-pressure 'TGiJOItS, and a rapid heating, convenient retention of the heat; and rapid cooling of the vessel'by confining the heating fluid to a space immediately adjacent to the interior walls of the vessel, from which it may be quickly displaced, thus avoiding having to heat and 0001' large masses of fire-brick as in the usual construc-' tion. I thereby increase the volume of output and avoid the cost of the otherwise necessa enclosing brickwork.

5 her advantages of the invention will appear in the course of the detailed description of the apparatus. 1

J In order that my said. invention may be clearly understood and readily carried into l0 effect, I will describe the same with reference to the accompanying drawings in which Figures 1, 2 and 3 show a rotatabletypeof apparatus provided with my preferred type of closure at one end only and in which figures like reference characters refer to like parts, while Figures 4 and 5'show a nonrotatable type of retort, and in which both ends are provided with identical breech mechanism closures.

Figure 1 is a side elevation and vertical longitudinal section of my rotary retort along the line A.B of Fig. 2, with the boiler covering omitted from the lower half of the retort and with the retort connection to condensation apparatus conventionally shown;

Figure 2 represents a rear end view of the retort and Figure 3 is a front end view of the latter, with a portion cut out to show the engagement of the rack and pinion. Figure 4 is a detail view of a non-rotatably mounted 'retort, partly in side elevation and partly in longitudinal section, and Figure 5 is an end view of one of the closures and its attached breech mechanism. 1 is the retort or still, comprising a preferably horizontally mounted tubular body 2, made of high-pressure resisting material, preferably drawn steel, with integral flanges 3 and 3 provided with a circular series of boltholes 4 and 4" at each end, and a shoulder portion 5 and 5 cut out from the inner edge'of each-flange for receiving a packing ring 6 and 6", preferably made of soft annealed copper.

. A rear cover: late or fermeture 7, shown in Figure 2, is astened to the flange 3 by means of nutted bolts 8, which are drawn so as to jam the packing ring 6" into the cutout1 portion 5 and. thus form a gas-tight sea To the outer central portion of the cover-' plate is screwed a fitting 9, preferably made of steel or bronze, provided with a lon itudinal bore 10 of small diameter for loose y receiving a needlevalve rod 1l, with its inner end portion adapted to fit tightly on the valve seat 11 provided in the center of the cover plate, and leading through an inwardly threaded stufling box 12 which is outwardly threaded into the fitting 9, and

is provided with threads and a handle 13.

Two horizontal bores 14 and 15, of small diameter, at right angles to the bore 10, lead to copper piping carrying controlling devices, to wit, a high-pressure gauge 16 on the left' and a spring safety valve 17 on the right. J

Whenever it..is desired to open the rear endof the retort, it is only necessary to remove the nuts from the bolts 8, grasp the fitting 9 and therewith lift off the cover plate from the body portion of the retort. Obviously the said fitting serves as a handle or means also for closing the rear end or fermeture of the retort. Instead of a cover plate the rear end of the autoclave, if desired, may be provided with identically the same fermeture as the front end of the retort, as is shown in the modified autoclave screw-threaded passage-way closed by an interrupted male screw plug 20, fastened to a ring 21, which is rotatably secured to a swingable carrier 22, which in turn may be rotated on the pivot bolt 23 by means of the hand lever 24, on which is pivoted one end of the link 25, which is hinged at its other end to the carrier ring 21, substantially as in standard breech mechanism.

In the central outer portion of the plug 22 is screwed a fitting 26, preferably made of steel or bronze, provided with a longitudinal bore 27,'of small diameter for loosely receiving a needle valve rod 28, adapted to fit on the valve seat 28, threaded and leading through a stuffing box 29, which is threaded into the fitting 26, and provided with a handle 30, and a vertical bore 31, leading to a nipple 32 and from Which a flexible copper tubing 33 connected by means of reducing couplings 34 and 35 and a-union 36, provided with a valve 37, leads to the ascension pipe 38 of the condensing apparatus, shown diagrammatically in part, and of well-known construction.

Surrounding the tubular body 2 at a suitable distance and bolted to its flanges 3 and 3 is a flanged sectional jacket 39, preferably of cast iron, provided with a manhole and cover 40 and 41 respectively, and a valve controlled inlet and outlet 42 and 43, respectively, for introducing and discharging the heating medium. Suitable for the last is molten lead, which may be heated so that the temperature of the retort will be maintained at about 4009 C, or alloys of low fusibility or hard paraffin, or even superheated steam, except when the highest temperatures are required.

Lossof heat by radiation is minimized by covering the jacket with a fibrous boiler covering 44.

The inner surface of the walls of the tubular body 2 may be protected particularly against the difi'usive and weakening action of hydrogen gas at high pressures and temperatures, by a tubular liner 45 of thin seamless copper expanded against the steel wall, or by protecting the latter by an electrodeposited metal or alloy or by a porcelain coating.

' The vessel 2 is rotatably mounted on preferably four ball-bearing rollers 46, 46 and 47, mounted on fixed journal bearings 48, 48 and 49, by. means of two tread bands 50 and 51 bolted to the jacket flanges 52 and 53, respectively.

Rotation is effected by means L of the toothed pinion 54, actuated by motor 55, and engaging the teeth of the circular rack 56, which is preferably located centrally in the transverse plane of the vessel and is bolted to the flanges 57 of the jacket.

. My apparatus is operated as follows, for example when hydrogenating peat, so as to secure valuable synthetic oils therefrom, although it is suitable for cheaply producing numerous other synthetic compounds at high pressures on a commercial scale.

Assuming the retort to be closed but empty, it is opened by swinging the lever 24 around outwardly so as to rotate the ring 21 far enough to disengage the screw threads of the plug 20 from its passage-way, and then to withdraw and swing out the plug clear of the headpiece so as to open the passage-way to admit of charging. The retort is now charged with a" mixture of about 500 lbs. of peat and 1000 lbs. of sodium formate, and the charging opening closed by returning the hand lever 24 to its original position.

The flexible connection of the retort with the condensing apparatus is disconnected, the needle valve comprising thev elements 28 and 28 closed and the needle valve rod 11 turned slightly so as to open the valve only so far as to allow of measuring the pressure in the retort and permitting of the operation of the safety valve in case of excessive pressure.

Molten lead, previously heated to about 430 (1, is now led into the-annular space of the jacket 39 by means of the pipe inlet 42, and the retort slowly rotated for a period of say 3 hours, while a temperature of about 400 C. and a pressure of approximately 100 atmospheres or 1500 lbs. per sq. in, as far as possible is maintained within the retort. The rotation of the vessel is now discontinued, the flexible copper tubing connection with the condensing apparatus established, and the fluid products of the react on allowed to escape into the ascension pipe by manipulating the needle valve rod 28. en the retort has cooled sufliciently, which cooling time may be shortene by letting the hot lead run out of the jac et and introduolng therein a suitable cooling medium, and the fluid products of thereaction I have all been collected, the retort is opened by means of the handlever 24 and the residue, chiefly sodium carbonate, removed from the retort. This completes the run of a .6 hour "shift and,the retort may now be recharged for a new run.

Referring now to Figures 4 and 5 of the drawing, 2 is a non-rotatably mounted retort, provided with a steam-jacket 2, or a space for holding a suitable heating medium, and closed at each end by fermeture plugs 3 and 3 -provided in the head-pieces or ja'ckets 4: and 4?, having passage ways with interrupted screw threads secured to the ends of' the body portion of the retort. Both fermetu-res are preferably of the interrupted screw thread breech-mechanism type, but any similar mechanism enabling the retort to be quickly and safely opened and closed gas-tight for high pressures'may be substituted. Asillustrated, the said mechanisms are manipulated in the usual way by hand-levers 5 and 5 to which are journaled links having a two-way motion and pivoted to rotatable and retractible carrier rings to which the plugs 3 and 3 provided with interrupted screw threads, are secured. Each breech plug is preferably tapped centrally and provided with a spindle blocl 6 and 6 threaded into the outer third of the plug, and having passage-ways 7 and 7 therein, and carrying a centrally placed needle valve 8 and 8*, each controlling its respective passage way, threaded I into. a bushing provided in the spindle block near its outer end. Flexible pipes 10 and 10 are coupled to the flanges provided on the outer ends of the passage ways 7 and .7' for connection with devices for supplying steam or gas or condensing apparatus.

It is to be understood that while I have specifically described the utilization of eat in my apparatus, other coal-like or bitumen-like materials, and substances such as alkali metal hydrate, may be combined with gaseous liquid or solid substances at high pressures and elevated temperatures in my apparatus in order to form valuable synthetic compounds.

What I claim as new is:

1. A retort comprising a double wall of tubular cross section, said wall enclosing an annular space for-retaining a heating or a cooling medium, a head piece on an end of said double wall provided with an opening .for charging and discharging solids, a plug fitting said opening, means for positively securing said plug on and releasing it from said head piece, and means secured to said double wall by which said retort may be rotated. 1

2. A retort comprising a double wall of tubular cross-section, a lining for the inner of said wallsimpervious to hydrogen gas,

a head piece on an end ofisaid double wall provided with an opening for charging and discharging solids, a plug fitting said opening an provided with a passage way for fluids, and means for positively securing said plug on and releasing it fromsaid head piece. I 3. A retort comprising a double wall of tubular cross section, said wall enclosing an annular space for retaining a heating or a coolin medium, a head piece on an end- ,of said ouble wall provided with an opening for charging and discharging solids, an interrupted screw mechanism mounted on said head piece and fitting said opening and a train of levers operatlvely connected with said screw mechanism for moving the same.

4. A retort comprising a double wall of tubular cross-section, a head piece on an end of said double wall provided with an opening for charging and discharging solids, a

vided with a passage way for fluids, a valve controlling the flow of fluids in said passage way, and means for positively securing said plug on and releasing it from said head plece.

6. A retort comprising a double wall of tubular cross section, a head piece on an end of said double wall provided with an opening for charging and discharging solids, said opening being provided with interrupted female screw threads, a plug provided with interrupted male threads for engaging said female threads when said opening is closed,,and mechanism for quickly dis-engaging said threads when said plug is to be Withdrawn.

7 In a normally closed retort, longitudinal metallic walls provided with means for preventing their undue weakening at high pressures and temperatures, an opening at one endof the retort for charging and discharging and provided with interrupted fetion, an interrupted screw closure disen- I gageably mounted in said head piece, a passage way for fluids in said closure, a valve for controlling the movement of said fluids in said passage Way, and lever means for manipulating said closure.

9. A retort comprising a tubularbody portion, a head piece for closing an end of said body portion, means for retaining gageably mounted on a circular opening in.

said head piece, interrupted screw threads provided in said opening, a carrier ring secured to said plug, and a system of levers connected tosaid carrier ring for engaging or disengaging said threads and Withdrawing said plug' TITUS ULKE 

